Development and validation of an UPLC-ESI-MS/MS method for determination of dehydroevodiamine, limonin, evodiamine, and rutaecarpine in Evodiae Fructus

Abstract

Objective:Evodiae Fructus (EF), one of the most widely used traditional Chinese medicines, mainly consists of alkaloids, is widely used for the treatments of headache and gastrointestinal disorders. In this study, a sensitive and reliable UPLC-ESI-MS/MS method was developed for qualitative determination of dehydroevodiamine, limonin, evodiamine, and rutaecarpine.Materials and Methods:Chromatographic separations were accomplished on a Phenomenex Kinetex XB-C18 column (2.1 × 150 mm, 1.7 μm) by using a gradient elution profile with a mobile phase consisting of 0.5% formic acid in water (A) and acetonitrile (B). Detection was performed using multiple reactions monitoring mode under ESI in the positive ion mode.Results:The results showed good linearity over the investigated concentration ranges (R2>0.9900) for the analytes. The limit of quantitations (LOQs) were 6.88 ng/mL for dehydroevodiamine, 18.6 ng/mL for limonin, 6.24 ng/mL for evodiamine, and 2.56 ng/mL for rutaecarpine, respectively. Intraday and interday precisions (relative standard deviations, %) were <5% and accuracies ranged from 92% to 106%.Conclusion:The validated method was successfully applied to assay the contents of the four compounds in EF samples from different regions, with which just 10 min was needed to analyze each sample.

Analysis ofE. rutaecarpaAlkaloids ConstituentsIn VitroandIn Vivoby UPLC-Q-TOF-MS Combined with Diagnostic Fragment

“…After we detected the alkaloids in E. rutaecarpa , we observed a high abundance of [M+H] + ion peaks in the excimer (+) ESI mass spectra, whereas [M−H] − signals nearly did not appear in the excimer (−) ESI mass spectra. Thus, mass spectrum in positive ion mode was finally obtained, which was consistent with the literature [ 23 ].…”

Chromatographic and mass spectrometric technologies for chemical analysis of Euodiae fructus: A review

“…Based on the satisfactory operational performance of the parent ion scan, the daughter ion scan, the neutral loss scan, selected reaction monitoring (SRM), and multiple reaction monitoring (MRM), together with the favorable characteristic of high selectivity and high signal-to-noise ratio (SNR), QQQ-MS is very suitable for the accurate determination of analyte contents, especially for trace constituents in complex systems, and the lowest value of the linear range easily reaches the nanolevel or even lower. Zhao et al 104 introduced an effective quantitative method based on a QQQ analyzer for rutaecarpine (1), evodiamine (5), dehydroevodiamine (8), and limonin (78) from 19 batches of Euodiae fructus samples. Determination was carried out using MRM in positive ion mode, providing limits of quantification (LOQs) from 2.56 to 18.6 ng/ml.…”

The pharmacokinetics profiles, pharmacological properties, and toxicological risks of dehydroevodiamine: A review

“…Due to higher polarity, DHE is the active compound in a higher yield in EF. Chromatographic separations revealed a limit of quantifications of 6.88 ng/ml for DHE in EF (Zhao et al, 2014). Modern researches confirm that DHE exerts extensive pharmacological activities in vitro and in vivo, such as antiinflammatory, anti-hypertensive, anti-cancer, anti-thrombotic, anti-obesity, anti-cholinesterase, anti-amnestic, analgesic, neuroprotective, and vasodilatory activities (Yang et al, 1990;Wang et al, 2001;Lim et al, 2004;Zhang Y. N. et al, 2018;Tian et al, 2019;Dai et al, 2022).…”